Chlorosulfonic acid → 4-((S)-2-Fluoro-1-methyl-ethyl)-benzenesulfonyl chloride

HRID 870336

반응식

HRID 870336 반응식
[F:1][CH2:2][C@H:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH3:4].[Cl:11][S:12](O)(=[O:14])=[O:13]>ClCCl>[F:1][CH2:2][C@H:3]([C:5]1[CH:10]=[CH:9][C:8]([S:12]([Cl:11])(=[O:14])=[O:13])=[CH:7][CH:6]=1)[CH3:4]

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 53628601((S)-2-Fluoro-1-methyl-ethyl)-benzene

생성물 1

HCID 536286004-((S)-2-Fluoro-1-methyl-ethyl)-benzenesulfonyl chloride수율 25%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
30 °C

실험 절차

3.5 g of ((S)-2-fluoro-1-methyl-ethyl)-benzene (25.32 mmol) were dissolved in 80 ml of dichloromethane. At 0-5° C., 11.81 g of chlorosulfonic acid (101.31 mmol), dissolved in 20 ml of dichloromethane, were added dropwise. The reaction mixture was stirred for 30 min at room temperature and 2 h at 30° C. The solvent was evaporated. 150 ml of diethyl ether were added to the residue, washed once with 150 ml water, and the organic layer was dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure. The crude product was purified via silica gel chromatography with n-heptane-dichloromethane (6:4) as eluent to give 1.5 g of the title compound.

후처리

  1. additionwere added dropwise
  2. customThe solvent was evaporated
  3. addition150 ml of diethyl ether were added to the residue
  4. washwashed once with 150 ml water
  5. dry with materialthe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customthe solvent evaporated under reduced pressure
  8. customThe crude product was purified via silica gel chromatography with n-heptane-dichloromethane (6:4) as eluent

출처 및 근거

ORD 기록
ord-782dc289896946e39552bcbe6e832e44
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969552B2

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